31 results about "Pyridine synthesis" patented technology

The invention provides a pyridine synthesis catalyst which takes microspherical high-silicon ZSM-5 molecular sieve as a carrier and a preparation method thereof. The preparation method adopts hydroxides of silicon source, aluminium source, alkali metal or alkaline earth metal, tetrapropylammonium bromide or tetrapropylammonium hydroxide and water as raw materials for preparing slurry, silicon-aluminum microspheres with the diameter of 30 to 200 um are obtained by spray drying and shaping, then the silicon-aluminum microspheres are arranged in organic amine steam, and the microspherical high-silicon ZSM-5 molecular sieve is obtained by washing, drying and calcination after the hydrothermal synthesis and the crystallization. The microspherical high-silicon ZSM-5 molecular sieve is taken as the carrier, one or more Pb, Sn and Zn elements is / are taken as main agents of active components, VIII family transition elements, IV family transition elements or / and alkaline earth metal elements are taken as auxiliary agents of the active components, wherein, the molar ratio of the total auxiliary agent to the total main agents is 0: 1 to 1: 1, the weight ratio of the active components and the carrier is 0.01 to 0.2; the carrier is impregnated in solution containing active components, and the catalyst of the invention is obtained by drying, calcination and activation, etc. As the synthesis process of the microspherical high-silicon ZSM-5 molecular sieve carrier which is used by the catalyst is shaped, the secondary shaping is unnecessary; at the same time, the catalyst can avoid the impact of a binding agent, thereby having better activity in applications. The yield of pyridine can achieve 77 percent and the total yield of pyridine derivatives can achieve 90 percent under the action of the catalyst. The catalyst of the invention is especially applicable to the fluidized bed catalytic process.

The invention discloses a supported catalyst for synthesizing pyridine with tetrahydrofurfuryl alcohol and discloses the method for preparation, belonging to the catalyst technique for synthesizing pyridine. Said carrier of the catalyst is gamma- A1203, one of supporter components is MoO3, the mass of which is 5- 30% to that of carrier, another supporter component is V205, the mass of which is 5- 30% to that of carrier, and the third is La, Ce or Cd oxide, the mass of which is 0.5- 15% to that of carrier. The technique contains the following steps: Dissolving ammonium molybdate, ammonium metavanadate and a nitrate containing La, Ce or Cd into water to prepare an ammonium molybdate solution and a nitrate solution, mixing the dried gamma- A1203, mixing to make sure that the solution is uniformly absorbed into the micropore of the carrier aluminum oxide, drying in room temperature; redrying the room- temperature dried catalyst and igniting to prepare the supported catalyst that is used to synthesize pyridine with tetrahydrofurfuryl alcohol. The device needed is simple, the production is convenient, and the selectivity and yield of product pyridine is high.

The invention discloses a method for treating pyridine wastewater, which comprises the following steps: pyridine wastewater, which is discharged from a pyridine extraction tower in an acetaldehyde+formaldehyde+liquid ammonia high-temperature pyridine synthesis technique, is subjected to low-vacuum flash distillation gas stripping, gas-phase absorption, fixed bed adsorption, desorption, distillation and other steps to separate and recover ammonia, pyridine and 3-methylpyridine in the pyridine wastewater, and the colorless water is subjected to biochemical treatment and discharged after reaching the standard. The method solves the problems of discharge of incinerator exhaust NOX, high incineration cost and carbon discharge due to abundant pyridine and derivatives in the wastewater incineration process in the pyridine production technique, effectively recovers the pyridine and derivatives, saves the cost, and lowers the pollution.

The invention provides a method for one-step direct preparation of 3-acyl imidazole [1, 5-a] pyridine through [4 + 1] ketomethyl secondary amination reaction, and the method comprises the following steps: electrolyzing 1 equivalent of R1-ethyl ketone, 2 equivalent of pyridine-2-R2-formamide and 1.5 equivalent of NH4I for 16-20 hours in a diaphragm-free electrolytic bath under the constant current condition of 10-25 mA to obtain a product. The efficient electrochemical synthesis method of 3-acyl imidazole [1, 5-a] pyridine is developed, and the conventional multi-step reaction of synthesis of 3-acylimidazole [1, 5-a] pyridine is avoided through two times of amination of cheap ketone methyl sp3 hydrocarbon; the direct synthesis method, the cheap materials, the simple metal-free system, no additional electrolyte or oxidant and expandability enable the method to become a practical and green method for preparing 3-acyl imidazole [1, 5-a] pyridine and a large pi-system.

The invention provides a pyridine synthesis catalyst which takes microspherical high-silicon ZSM-5 molecular sieve as a carrier and a preparation method thereof. The preparation method adopts hydroxides of silicon source, aluminium source, alkali metal or alkaline earth metal, tetrapropylammonium bromide or tetrapropylammonium hydroxide and water as raw materials for preparing slurry, silicon-aluminum microspheres with the diameter of 30 to 200 um are obtained by spray drying and shaping, then the silicon-aluminum microspheres are arranged in organic amine steam, and the microspherical high-silicon ZSM-5 molecular sieve is obtained by washing, drying and calcination after the hydrothermal synthesis and the crystallization. The microspherical high-silicon ZSM-5 molecular sieve is taken as the carrier, one or more Pb, Sn and Zn elements is / are taken as main agents of active components, VIII family transition elements, IV family transition elements or / and alkaline earth metal elements are taken as auxiliary agents of the active components, wherein, the molar ratio of the total auxiliary agent to the total main agents is 0: 1 to 1: 1, the weight ratio of the active components and the carrier is 0.01 to 0.2; the carrier is impregnated in solution containing active components, and the catalyst of the invention is obtained by drying, calcination and activation, etc. As the synthesis process of the microspherical high-silicon ZSM-5 molecular sieve carrier which is used by the catalyst is shaped, the secondary shaping is unnecessary; at the same time, the catalyst can avoid the impact of a binding agent, thereby having better activity in applications. The yield of pyridine can achieve 77 percent and the total yield of pyridine derivatives can achieve 90 percent under the actionof the catalyst. The catalyst of the invention is especially applicable to the fluidized bed catalytic process.

The invention discloses a novel SBQ sensitizer synthesizing method. 4-bromomethyl pyridine synthesis and Wittig reagent synthesis are separately carried out. Under the protection of N2, NaOH aqueous solution is added in a reaction container. The Wittig reagent and terephthalaldehyde undergo magnetic stirring and 12-hour circumfluence at 25 DEG C. HCL solution is added. A claret-red solution is obtained after filtration. reduced pressure distillation is carried out to remove the HCL solution. Brick red solid, i.e. 4-[2-4-formoxphenyl] vinyl] pyridine, i.e. SBQ sensitizer is obtained after drying. SBQ sensitive glue can be prepared from the SBQ sensitizer together with accessory agents such as polyvinyl alcohol, colorant and the like according to different proportions. According to tests, 15,000 times of printing can be stood by the SBQ sensitive glue, and the printing absolution is as high as 96 percent, which is equal to an imported product.

The present invention relates to a class of cypermeline analogs, a method for synthesizing the same and the use for inhibiting the activity of acetylcholinesterase. The preparation method of the described hemipramine analogue is based on 9-methyl-1,2,3,4,9,9a-6 hydrogen-4aH-pyrido[2,3-b]indole-4a- Alcohol is the substrate, add anhydrous pyridine to dissolve, slowly drop the reaction reagent organic acid or acid anhydride, after the reaction is complete, add a quenching agent to quench the reaction, and concentrate under reduced pressure to remove methanol and pyridine. The synthesis process is simple and the product purity is high. Inhibits acetylcholinesterase activity.

The invention discloses a preparation method of a hydroxyl pyridine compound, which comprises the following steps of: taking hydrochloride or sulfate or nitrate of alkyl guanidine (shown in the formula II) as a reaction raw material; neutralizing with sodium hydroxide or potassium hydroxide; and then, taking toluene or xylene or chlorobenzene as a reaction solvent, and taking methanol or ethanol as a cosolvent for refluxing, dehydrating and dealcoholizing with alpha-alkyl acetoacetic ester (shown in the formula III) to react to obtain the hydroxyl pyridine compound (shown in the formula I). In the invention, by adding the methanol or ethanol as the cosolvent in the hydroxyl pyridine synthesis reaction, the solubility of the alkyl guanidine can be well increased, the decomposition of the reactants (alpha-alkyl acetoacetic ester and alkyl guanidine) is effectively controlled, the formation rate of the target product namely the hydroxyl pyridine compound shown in the general formula (I) is greatly increased, and the yield and content of the hydroxyl pyridine compound product shown in the general formula (I) are obviously improved, wherein the product yield is greater than 94%, and the product content is greater than 97%.

The invention belongs to the field of medicinal chemistry and relates to a preparation technology of 2-methoxy-5-(pyridine-2-yl)pyridine as a perampanel intermediate. The preparation technology comprises that 5-bromo-2-methoxypyridine and bis(pinacolato)diboron undergo a reaction to produce 2-methoxypyridine-5-boronic acid pinacol ester and the 2-methoxypyridine-5-boronic acid pinacol ester and 2-halogenated pyridine undergo a reaction to produce 2-methoxy-5-(pyridine-2-yl)pyridine as a perampanel intermediate. The synthesis method solves the problem of a high catalyst cost, has the advantages of simple processes and low cost and is convenient for large scale production.

The present invention discloses a 2-chloro-5-ethyl pyridine synthesis method. According to the method, a Suzuki reaction is performed to convert 2-chloro-5-bromopyridine into 2-chloro-5-vinylpyridine, or a Wittig reaction is performed to convert 2-chloro-5-formyl pyridine into 2-chloro-5-vinylpyridine, and further an iridium-containing catalyst having a structure represented by a formula (I) is adopted to carry out selective hydrogenation to convert the 2-chloro-5-vinylpyridine into the 2-chloro-5-ethyl pyridine, wherein R is cyclohexyl, n-butyl or phenyl, and L is pyridine or unsaturated nitrogen-containing carbene. The method of the present invention has advantages of high selectivity, high yield and convenient purification. The formula (I) is defined in the instruction.

The invention discloses a method for synthesizing indene ketone and imidazole and pyridine compounds. The method comprises the steps that 2-(2- bromophenyl) imidazole [1, 2-alpha] pyridine or a derivative thereof is dissolved in solvent, then catalysts, ligands and alkali are added, a reaction is conducted in oil bath at the temperature of 120-160 DEG C under the atmosphere of 1atm of CO, and the 11H-indene [1', 2': 4, 5] imidazole [1, 2-alpha] pyridine-11-ketone compounds are obtained. The synthesis process is simple and efficient, a series-connection reaction under catalysis of transition metal is utilized, the indene ketone and imidazole and pyridine compounds are obtained through one step, in other words, an indene ketone structure is constructed while indanone and an imidazole and pyridine structural unit are linked together, resource waste and environmental pollution caused by application of multiple types of reagent andpurification treatment of the ligands in all steps of the reaction and the like in multiple steps of the reaction are avoided, raw materials are easy to prepare, the reaction is easy and convenient to operate, and the adaptability range of a substrate is wide.

The invention relates to a synthesis method of a 2-substituted pyridine-class drug intermediate compound shown in the formula (I) (please see the formula in the specification). The method includes the steps that when catalysts, ligand, alkali and additives exist, a compound with the formula (II) and a compound with the formula (III) react in an organic solvent so that the compound shown in the formula (I) (please see the formula in the specification) can be obtained, wherein R1, R2 and R3 are independently selected from H, halogen or C-C6 alkyl groups; the formula (please see the formula in the specification) is a C6-C10 aryl group which is not substituted or has 1-2 substitutent groups or is a C4-C10 heterocyclic radical which is not substituted or has 1-2 substitutent groups, and the substitutent grous are halogen, nitro or C1-C6 alkyl groups; Hal serves as the halogen. According to the method, the catalysts, the ligand, the alkali and the additives are properly selected and combined, and therefore a high yield is achieved, and the method has good industrial prospects and good application potentiality.

Synthesis of micron and nanometer particle containing Ru(bpy)32+ is carried out by mixing Ru(bpy)32+ with anionic compound or anionic polyelectrolyte solution proportionally and preparing mass micron and nanometer particle containing Ru(bpy)32+. It has excellent electrochemiluminescent performance and is simple and fast. It can be used for capillary electrophoresis or solid ECL inspection.

The invention discloses a method for synthesizing ketones or aldehydes by catalyzing the oxidation of pyridine compounds by manganese compounds. Pyridine compounds containing substituents are used as reaction substrates, manganese compounds are used as catalysts, and water, tert-butanol, acetonitrile, ethyl acetate or One or more than two kinds of dichloromethane as solvent, peroxide as oxygen source, react at 25-50°C for 12-48 h, so that the C-H bond of pyridine side chain is oxidized into ketone or aldehyde in one step, and the reaction The crude product was processed to obtain the final product. The preparation method of the invention has mild reaction conditions, less catalyst consumption, high atom economy, simple operation, wide application range of substrates and industrial applicability.

The invention discloses a supported catalyst for synthesizing pyridine with tetrahydrofurfuryl alcohol and discloses the method for preparation, belonging to the catalyst technique for synthesizing pyridine. Said carrier of the catalyst is gamma- A1203, one of supporter components is MoO3, the mass of which is 5- 30% to that of carrier, another supporter component is V205, the mass of which is 5- 30% to that of carrier, and the third is La, Ce or Cd oxide, the mass of which is 0.5- 15% to that of carrier. The technique contains the following steps: Dissolving ammonium molybdate, ammonium metavanadate and a nitrate containing La, Ce or Cd into water to prepare an ammonium molybdate solution and a nitrate solution, mixing the dried gamma- A1203, mixing to make sure that the solution is uniformly absorbed into the micropore of the carrier aluminum oxide, drying in room temperature; redrying the room- temperature dried catalyst and igniting to prepare the supported catalyst that is used to synthesize pyridine with tetrahydrofurfuryl alcohol. The device needed is simple, the production is convenient, and the selectivity and yield of product pyridine is high.

The invention relates to a synthesizing process of 5-bromo-3-methyl-1H-pyrazolo [3, 4-B] pyridine. The synthesizing process comprises the following steps: 5-bromine-3-acetenyl-2-chlorine-pyridine is dissolved into DMF, then hydrazine, calcium carbonate and aluminium silicate are added sequentially and mixed uniformly, the mixture is reacted for 24-36 hours at the temperature of 1 DEGC to 10 DEG C, insoluble substances are filtered, the pressure is reduced to steam a solvent, and ethyl alcohol is used for recrystallization, so that the 5-bromo-3-methyl-1H-pyrazolo [3, 4-B] pyridine can be obtained. According to the synthesizing process, the aluminium silicate is used as a catalyst, so that the operation steps are simple, the yield is higher and industrial large-scale production of the 5-bromo-3-methyl-1H-pyrazolo [3, 4-B] pyridine is facilitated.